反应详情

To 3.0 g (21 mmol) of benzoyl acetonitrile in 50 mL of THF, cooled in a wet ice bath, was added 0.84 g (21 mmol) of sodium hydride (60% oil dispersion). After 1 h, added 2.8 g (10 mmol) of 3-bromoacetylpyridine hydrobromide. After 3 h, poured the reaction mixture into brine, extracted with ethyl acetate, dried over sodium sulfate, concentrated under reduced pressure and purified by flash chromatography (gradient elution: 40-80% ethyl acetate/hexane) to give 2.6 g (93%) of 2-benzoyl-4-oxo-4-pyridin-3-yl-butyronitrile (MH+=265).

1. waitAfter 3 h
2. extractionextracted with ethyl acetate
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. custompurified by flash chromatography (gradient elution: 40-80% ethyl acetate/hexane)